CN108085783A - High tenacity carborundum and preparation method thereof - Google Patents
High tenacity carborundum and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to high tenacity carborundum and preparation method thereof, and described method includes following steps:Ferroso-ferric oxide and metallic cobalt ball milling are dissolved in into particle, then by particle in isopropanol and the mixed solution of deionized water;Product is dried, and is ultrasonically treated after being mixed with poly dimethyl silicon borine, is then dissolved in isopropanol and stirs;Product is subjected to cure treatment, obtains high tenacity carborundum.The preparation method of the high tenacity carborundum of the present invention, ferroso-ferric oxide and cobalt powder are introduced in the preparation process of silicon carbide fibre, utilize the magnetism of ferroso-ferric oxide, nano-cobalt powder is adsorbed in the preparation, the crackle that material surface occurs when high temperature prepares carborundum is filled up, extra cobalt powder forms cobalt silicide with silicon at high temperature, forms stable structure, enhances the performance of carborundum.Thus the silicon carbide fibre face crack prepared is few, and toughness is big, stable performance under high temperature, and good application prospect is presented in aerospace high-temperature field.
Description
Technical field
The invention belongs to field of material technology, and in particular to high tenacity carborundum and preparation method thereof.
Background technology
Silicon carbide ceramics is navigating because of its excellent elevated temperature strength, wearability, corrosion resistance and good conductive, thermal conductivity
Numerous industries such as empty space flight, machinery, automobile are used widely.Simultaneously it be also military field important materials, developed country
Technology blockage is carried out to China, so China must independently develop the silicon carbide fibre haveing excellent performance, China could be improved
Military strength and overall national strength.
But silicon carbide ceramics brittleness is larger, fracture toughness is relatively low, and normal pressure-sintered silicon carbide ceramics flexural strength is general
In 400MPa or so, it is difficult to meet demand of the fields such as sealing, armoring industry to the silicon carbide ceramics of high tenacity, high intensity.
The content of the invention
An object of the present invention is to provide a kind of preparation methods of high tenacity carborundum.
A kind of preparation method of high tenacity carborundum of the present invention, includes the following steps:S101:By ferroso-ferric oxide and gold
Belong to cobalt mixing, then ball milling into 30nm~40nm particle, then the particle is dissolved in isopropanol and deionized water mixing it is molten
In liquid;Wherein, the mass ratio of the ferroso-ferric oxide and the metallic cobalt is (2~5):1;S102:The step S101 is obtained
The product drying arrived, obtains the solid powder of fluidized state;S103:The solid powder that the step S102 is obtained and poly- diformazan
It is ultrasonically treated after the mixing of base silicon borine, is then dissolved in isopropanol and stirs;Wherein, the poly dimethyl silicon borine and institute
The mass ratio for stating solid powder is (5~10):(1~3), the gross mass of the poly dimethyl silicon borine and the solid powder with
The mass ratio of the isopropanol is 1:(5~10);S104:The product that the step S103 is obtained carries out non-fusible in air
1h~1.5h is handled, then cure treatment 5h~6h will be carried out in its again vacuum, nano-cobalt powder is added and continues non-fusible place
Manage 1h~1.5h;Wherein, the mass ratio of the ferroso-ferric oxide in the product that the nano-cobalt powder and the step S103 are obtained is
(3~6):(1~2);S105:Under protective gas atmosphere, the obtained products of the step S104 are put into tube furnace, then
800 DEG C~1000 DEG C are warming up under the first heating rate, and keeps the temperature 2h~3h, is then warming up under the second heating rate
1500 DEG C~1600 DEG C, and 2h~3h is kept the temperature, room temperature then is dropped in the first rate of temperature fall, obtains high tenacity carborundum.
The preparation method of the high tenacity carborundum of the present invention, ferroso-ferric oxide is introduced in the preparation process of silicon carbide fibre
And cobalt powder, using the magnetism of ferroso-ferric oxide, nano-cobalt powder is adsorbed in the preparation, has filled up material table when high temperature prepares carborundum
The crackle that face occurs, extra cobalt powder with forming cobalt silicide with silicon, form stable structure, enhance carborundum at high temperature
Performance.Thus the silicon carbide fibre face crack prepared is few, and toughness is big, stable performance under high temperature, is led in aerospace high temperature
Domain presents good application prospect.
In addition, the preparation method of high tenacity carborundum according to the above embodiment of the present invention, can also have following additional
Technical characteristic:
Further, in the step S101, the ferroso-ferric oxide and the isopropanol and the mass ratio of the water
For 1:(0.5~1):(10~20).
Further, in the step S102, drying time is 5h~10h, and drying temperature is 50 DEG C~80 DEG C.
Further, in the step S103, the time of supersound process is 1h~2h.
Further, in the step S103, mixing time is 5h~10h.
Further, in the step S105, the first heating rate be 200 DEG C/h~300 DEG C/h, described second
Heating rate is 300 DEG C/h~400 DEG C/h, and first rate of temperature fall is 500 DEG C/h~550 DEG C/h.
Further, in the step S105, the protective gas is argon gas, and the flow of the argon gas is 300mL/
Min~400mL/min.
It is another object of the present invention to the high tenacity carborundum for proposing to be prepared with the method.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
It obtains substantially or is recognized by the practice of the present invention.
Specific embodiment
The embodiment of the present invention is described below in detail, the embodiment is exemplary, it is intended to for explaining the present invention, and
It is not considered as limiting the invention.
Embodiment 1
Embodiment 1 proposes a kind of high tenacity carborundum, and its preparation method includes the following steps:
(1) ferroso-ferric oxide is mixed with metallic cobalt, then the particle then is dissolved in isopropyl by ball milling into the particle of 30nm
In alcohol and the mixed solution of deionized water;Wherein, the mass ratio of the ferroso-ferric oxide and the metallic cobalt is 2:1;Described four
Fe 3 O is 1 with the mass ratio of the isopropanol and the water:1:10.
(2) product for obtaining the step (1) dry 5h at a temperature of 80 DEG C, obtains the solid powder of fluidized state.
(3) 2h is ultrasonically treated after the solid powder that the step (2) obtains is mixed with poly dimethyl silicon borine, then will
It is dissolved in isopropanol and stirs 5h;Wherein, the mass ratio of the poly dimethyl silicon borine and the solid powder is 10:1, institute
It is 1 that poly dimethyl silicon borine, which is stated, with the gross mass of the solid powder and the mass ratio of the isopropanol:10.
(4) product that the step (3) obtains is subjected to cure treatment 2h in air, then by its again vacuum into
Row cure treatment 6h adds nano-cobalt powder and continues cure treatment 1h;Wherein, the nano-cobalt powder and the step (3)
The mass ratio of ferroso-ferric oxide in obtained product is 6:1.
(5) under argon atmosphere, the product that the step (5) obtains is put into tube furnace, then in the liter of 300 DEG C/h
800 DEG C are warming up under warm rate, and keeps the temperature 3h, 1600 DEG C are then warming up under the heating rate of 300 DEG C/h, and keeps the temperature 2h,
Then room temperature is dropped in the rate of temperature fall of 550 DEG C/h, obtains high tenacity carborundum.Wherein, the flow of the argon gas is
300mL/min。
Embodiment 2
Embodiment 2 proposes a kind of high tenacity carborundum, and its preparation method includes the following steps:
(1) ferroso-ferric oxide is mixed with metallic cobalt, then the particle then is dissolved in isopropyl by ball milling into the particle of 40nm
In alcohol and the mixed solution of deionized water;Wherein, the mass ratio of the ferroso-ferric oxide and the metallic cobalt is 3:1;Described four
Fe 3 O is 1 with the mass ratio of the isopropanol and the water:0.5:20.
(2) product for obtaining the step (1) dry 10h at a temperature of 50 DEG C, obtains the solid powder of fluidized state.
(3) 1h is ultrasonically treated after the solid powder that the step (2) obtains is mixed with poly dimethyl silicon borine, then will
It is dissolved in isopropanol and stirs 10h;Wherein, the mass ratio of the poly dimethyl silicon borine and the solid powder is 5:3, institute
It is 1 that poly dimethyl silicon borine, which is stated, with the gross mass of the solid powder and the mass ratio of the isopropanol:5.
(4) product that the step (3) obtains is subjected to cure treatment 3h in air, then by its again vacuum into
Row cure treatment 5h adds nano-cobalt powder and continues cure treatment 1.2h;Wherein, the nano-cobalt powder and the step
(3) mass ratio of the ferroso-ferric oxide in the product obtained is 3:2.
(5) under argon atmosphere, the product that the step (5) obtains is put into tube furnace, then in the liter of 200 DEG C/h
1000 DEG C are warming up under warm rate, and keeps the temperature 2h, 1500 DEG C are then warming up under the heating rate of 400 DEG C/h, and keeps the temperature 3h,
Then room temperature is dropped in the rate of temperature fall of 500 DEG C/h, obtains high tenacity carborundum.Wherein, the flow of the argon gas is
400mL/min。
Embodiment 3
Embodiment 3 proposes a kind of high tenacity carborundum, and its preparation method includes the following steps:
(1) ferroso-ferric oxide is mixed with metallic cobalt, then the particle then is dissolved in isopropyl by ball milling into the particle of 35nm
In alcohol and the mixed solution of deionized water;Wherein, the mass ratio of the ferroso-ferric oxide and the metallic cobalt is 5:1;Described four
Fe 3 O is 1 with the mass ratio of the isopropanol and the water:0.8:15.
(2) product for obtaining the step (1) dry 7.5h at a temperature of 65 DEG C, obtains the solid powder of fluidized state
End.
(3) 1.5h is ultrasonically treated after the solid powder that the step (2) obtains is mixed with poly dimethyl silicon borine, then
It is dissolved in isopropanol and stirs 7.5h;Wherein, the mass ratio of the poly dimethyl silicon borine and the solid powder is 4:
1, the poly dimethyl silicon borine is 1 with the gross mass of the solid powder and the mass ratio of the isopropanol:8.
(4) product that the step (3) obtains is subjected to cure treatment 2h in air, then by its again vacuum into
Row cure treatment 5.5h adds nano-cobalt powder and continues cure treatment 1.5h;Wherein, the nano-cobalt powder and the step
(3) mass ratio of the ferroso-ferric oxide in the product obtained is 4:1.
(5) under argon atmosphere, the product that the step (5) obtains is put into tube furnace, then in the liter of 250 DEG C/h
900 DEG C are warming up under warm rate, and keeps the temperature 2.5h, 1550 DEG C are then warming up under the heating rate of 350 DEG C/h, and is kept the temperature
Then 2.5h drops to room temperature in the rate of temperature fall of 520 DEG C/h, obtain high tenacity carborundum.Wherein, the flow of the argon gas is
350mL/min。
The preparation method of the high tenacity carborundum of the present invention, ferroso-ferric oxide is introduced in the preparation process of silicon carbide fibre
And cobalt powder, using the magnetism of ferroso-ferric oxide, nano-cobalt powder is adsorbed in the preparation, has filled up material table when high temperature prepares carborundum
The crackle that face occurs, extra cobalt powder with forming cobalt silicide with silicon, form stable structure, enhance carborundum at high temperature
Performance.Thus the silicon carbide fibre face crack prepared is few, and toughness is big, stable performance under high temperature, is led in aerospace high temperature
Domain presents good application prospect.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms is not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It is combined in an appropriate manner in one or more embodiments or example.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the different embodiments described in this specification or example and different embodiments or exemplary feature
It closes and combines.
Although the embodiment of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (8)
1. a kind of preparation method of high tenacity carborundum, which is characterized in that include the following steps:
S101:Ferroso-ferric oxide is mixed with metallic cobalt, then the particle then is dissolved in by ball milling into the particle of 30nm~40nm
In isopropanol and the mixed solution of deionized water;Wherein, the mass ratio of the ferroso-ferric oxide and the metallic cobalt is (2~5):
1;
S102:The product that the step S101 is obtained is dried, and obtains the solid powder of fluidized state;
S103:It is ultrasonically treated after the solid powder that the step S102 is obtained is mixed with poly dimethyl silicon borine, then by it
It is dissolved in isopropanol and stirs;Wherein, the mass ratio of the poly dimethyl silicon borine and the solid powder is (5~10):(1
~3), the poly dimethyl silicon borine and the gross mass of the solid powder and the mass ratio of the isopropanol are 1:(5~10);
S104:The obtained products of the step S103 are subjected to cure treatment 2h~3h in air, then by its vacuum again
Middle progress cure treatment 5h~6h adds nano-cobalt powder and continues cure treatment 1h~1.5h;Wherein, the nano-cobalt powder
The mass ratio of ferroso-ferric oxide in the product obtained with the step S103 is (3~6):(1~2);
S105:Under protective gas atmosphere, the obtained products of the step S104 are put into tube furnace, then in the first heating
800 DEG C~1000 DEG C are warming up under rate, and keeps the temperature 2h~3h, 1500 DEG C~1600 are then warming up under the second heating rate
DEG C, and 2h~3h is kept the temperature, room temperature then is dropped in the first rate of temperature fall, obtains high tenacity carborundum.
2. the preparation method of high tenacity carborundum according to claim 1, which is characterized in that in the step S101,
The ferroso-ferric oxide is 1 with the mass ratio of the isopropanol and the water:(0.5~1):(10~20).
3. the preparation method of high tenacity carborundum according to claim 1, which is characterized in that in the step S102,
Drying time is 5h~10h, and drying temperature is 50 DEG C~80 DEG C.
4. the preparation method of high tenacity carborundum according to claim 1, which is characterized in that in the step S103,
The time of supersound process is 1h~2h.
5. the preparation method of high tenacity carborundum according to claim 1, which is characterized in that in the step S103,
Mixing time is 5h~10h.
6. the preparation method of high tenacity carborundum according to claim 1, which is characterized in that in the step S105,
The first heating rate is 200 DEG C/h~300 DEG C/h, and second heating rate is 300 DEG C/h~400 DEG C/h, described the
One rate of temperature fall is 500 DEG C/h~550 DEG C/h.
7. the preparation method of high tenacity carborundum according to claim 1, which is characterized in that in the step S105,
The protective gas is argon gas, and the flow of the argon gas is 300mL/min~400mL/min.
8. the high tenacity carborundum prepared using claim 1-7 any one of them method.
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CN115385706A (en) * | 2022-08-23 | 2022-11-25 | 广西三元华鑫特种陶瓷有限公司 | Method for improving impact toughness of micro-nano fiber reinforced silicon carbide material |
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T. FUJIMURA等: "In-situ high temperature X-ray diffraction study of Co/SiC interface reactions", 《JOURNAL OF MATERIALS SCIENCE》 * |
王军 等: "聚碳硅烷/纳米钴粉的热裂解研究", 《材料科学与工程》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115385706A (en) * | 2022-08-23 | 2022-11-25 | 广西三元华鑫特种陶瓷有限公司 | Method for improving impact toughness of micro-nano fiber reinforced silicon carbide material |
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